CN114958290B - Organic silicon pressure-sensitive adhesive and preparation method and application thereof - Google Patents

Organic silicon pressure-sensitive adhesive and preparation method and application thereof Download PDF

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CN114958290B
CN114958290B CN202210517444.7A CN202210517444A CN114958290B CN 114958290 B CN114958290 B CN 114958290B CN 202210517444 A CN202210517444 A CN 202210517444A CN 114958290 B CN114958290 B CN 114958290B
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sensitive adhesive
pressure
parts
vinyl
resin
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CN114958290A (en
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徐燕芬
刘爱伟
彭川
张敏
曹峰
王金水
李强
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Meishan Tuoli Technology Co ltd
Chengdu Taly Technology Co ltd
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Chengdu Taly Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/20—Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22—Plastics; Metallised plastics
    • C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
    • C09J7/255—Polyesters
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C09J7/38—Pressure-sensitive adhesives [PSA]
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/40—Adhesives in the form of films or foils characterised by release liners
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
    • C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
    • C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2301/00—Additional features of adhesives in the form of films or foils
    • C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
    • C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2467/00—Presence of polyester
    • C09J2467/006—Presence of polyester in the substrate
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Adhesive Tapes (AREA)

Abstract

The invention belongs to the field of organic silicon pressure-sensitive adhesives, and relates to an organic silicon pressure-sensitive adhesive for an AF screen protection film and a preparation method thereof. The invention provides an organic silicon pressure-sensitive adhesive, which comprises a main agent component, a catalyst component, a cross-linking agent component and an anchoring agent component; the main agent comprises the following raw materials: vinyl polysiloxane, MQ resin, auxiliary agent, solvent and inhibitor, wherein the vinyl polysiloxane is composed of 2-20wt% of vinyl polysiloxane with vinyl content of 1.0-2.0wt% and 80-98wt% of vinyl polysiloxane with vinyl content of 0.03-0.2wt%; the MQ resin is composed of 70-90 wt% of methyl MQ resin and 10-30 wt% of vinyl MQ resin. The organic silicon pressure-sensitive adhesive has the film tearing force not more than 3.5g/25mm, has good aging stability, and can eliminate pause marks and fingerprint marks in a short time.

Description

Organic silicon pressure-sensitive adhesive and preparation method and application thereof
Technical Field
The invention belongs to the technical field of organic silicon pressure-sensitive adhesives, and particularly relates to an organic silicon pressure-sensitive adhesive for an AF screen protection film and a preparation method thereof.
Background
The organic silicon material has a special molecular structure and a soft and freely rotatable siloxane main chain, so that the material is endowed with excellent high and low temperature resistance, weather resistance and electrical property, and is widely applied to industries such as electronics, aerospace, military industry and the like. Similarly, the organosilicon material, as a pressure-sensitive adhesive, also has properties that other materials are difficult to possess: (1) The adhesive has good adhesion to high-energy and low-energy surface materials, and good adhesion to untreated materials difficult to adhere, such as polytetrafluoroethylene, polyimide, polycarbonate and the like; (2) The adhesive has excellent high and low temperature resistance, can be used for a long time at the temperature of between 50 ℃ below zero and 150 ℃, and still keeps good adhesive strength and flexibility at high temperature and low temperature; (3) has good chemical inertness and long service life; (4) Good chemical resistance and outstanding solvent and electrical properties; (5) no corrosion to metals; (6) dielectric properties are good. These excellent properties enable the organosilicon pressure-sensitive adhesive to be rapidly developed in the protective film industry, especially in the mobile phone screen and electronic display screen protective film industry, and the organosilicon pressure-sensitive adhesive occupies more than 90% of market share with the excellent properties.
An AF screen (anti-finger screen) is an anti-fingerprint high-definition display screen, and a layer of anti-fingerprint coating (a coating is generally a fluorine modified organic coating) is coated on the surface layer of a high-definition glass screen, so that the surface of the glass has very low surface tension, thereby having the effects of water resistance, oil resistance and fingerprint resistance. With the development of mobile phones and electronic industries, AF screens are widely applied in the mobile phone industry. According to the use habit of the mobile phone, people prefer to paste a layer of protective film on the surface layer of the mobile phone screen to prevent the screen with higher price from being damaged due to accidents, so that the pressure-sensitive adhesive for the AF screen is introduced in the market. However, due to the specificity of the AF screen surface coating, the stripping force of the conventional organic silicon pressure-sensitive adhesive to the AF screen is poor, and even the pressure-sensitive adhesive with the highest stripping force of the steel plate is generally less than 15g/25mm.
Early pressure-sensitive adhesives for AF screens were mainly pursued for peeling force to AF screens, and other indexes were correspondingly less required. However, with the improvement of the quality level of the AF screen, such as the increase of the water drop angle, the improvement of the surface hardness and the compactness, the development of the pure mechanical screen pasting technology, and the like, the early product with high AF screen stripping force cannot solve all the problems facing the market.
Firstly, through years of development, the technical level of the AF screen is greatly improved, and the water drop angle is also improved to more than 115 degrees from about 100 degrees at first, which is a main index for improving the performance of the AF screen. With the improvement of the water drop angle of the AF screen, the AF screen stripping force of the pressure-sensitive adhesive on the surface of the AF screen can be correspondingly reduced, the AF screen stripping force requirement of the pressure-sensitive adhesive can be met in early stage, and the AF screen stripping force of the pressure-sensitive adhesive at the current stage can be reduced or unqualified.
Secondly, the mobile phone film produced at present is mostly mechanically operated to replace the traditional manual film, which puts a new requirement on the film tearing force of the pressure sensitive adhesive and needs to be stable and within a certain range. Early-stage fluorine release films mainly depend on imported several varieties, and have stable performance, higher price, better matching property of pressure-sensitive adhesive and fluorine release films and stable film tearing force. However, with the increase of recombination and competition in the mobile phone market, the cost pressure is also increasing, and the cost of the fluorine release film is one of the main cost expenses in the pressure-sensitive adhesive composition for the AF screen, which must be greatly reduced. This provides a potential opportunity for the domestic fluoride release film market. However, the domestic fluoride release film market has the phenomena of various varieties and good performance, and the large-scale application of the domestic fluoride release film greatly reduces the cost, but the matching property with the pressure-sensitive adhesive for the AF screen is poor (the film tearing force is higher and unstable), so that the pressure-sensitive adhesive with good matching property with most of the main fluoride release films must be developed for matching use.
In addition, in the use process of the AF screen, considering that reworking sticking or fingernail scratching to the surface layer may occur in actual use, it is required that pause marks and fingerprint marks must disappear in a short time, otherwise, the use feeling and the product appearance of a user are affected.
Chinese patent CN201910130883.0 discloses a method for preparing an organosilicon pressure-sensitive adhesive for AF anti-fingerprint screen, the prepared organosilicon pressure-sensitive adhesive can be coated on PET, PI, PC base materials, and has high peeling force to AF anti-fingerprint screen, which can reach 60g/25mm; the stripping force does not change obviously with time (the stripping force is high and stable), and the stripping force is within 8g/25mm for the release film; the prepared organic silicon pressure-sensitive adhesive of the AF fingerprint-resistant screen has high strength, good stability to the peeling force of the AF screen, no attenuation, good adhesive force and no degumming after 2 hours of boiling resistance. However, the patent does not relate to indexes such as heating aging, fingerprint marks, pause marks and the like, and the film tearing force is 8g/25mm, so that the film tearing force cannot meet the requirement of not more than 3.5g/25 mm.
Disclosure of Invention
In view of the above-mentioned drawbacks, the present invention aims to provide an organosilicon pressure-sensitive adhesive for an AF screen protective film and a preparation method thereof, which solve the problems set forth in the above-mentioned background art by improving the direction of vinyl distribution and vinyl content design, MQ resin selection and collocation, and auxiliary agent selection of vinyl polysiloxane in a raw material formulation. The obtained organosilicon pressure-sensitive adhesive has a tearing force of not more than 3.5g/25mm, has good aging stability, and can eliminate pause marks and fingerprint marks in a short time.
The technical scheme of the invention is as follows:
the first technical problem to be solved by the invention is to provide an organic silicon pressure-sensitive adhesive, wherein the organic silicon pressure-sensitive adhesive comprises a main agent component, a catalyst component, a cross-linking agent component and an anchoring agent component; the main agent comprises the following raw materials: vinyl polysiloxane, MQ resin, auxiliary agent, solvent and inhibitor, wherein the vinyl polysiloxane is composed of 2-20wt% of vinyl polysiloxane with vinyl content of 1.0-2.0wt% and 80-98wt% of vinyl polysiloxane with vinyl content of 0.03-0.2wt%; the MQ resin is composed of 70-90 wt% of methyl MQ resin and 10-30 wt% of vinyl MQ resin.
Further, the auxiliary agent is a chain extension auxiliary agent.
Still further, the auxiliary agent is at least one of long-chain alkyl silicone oil, hydrogen-terminated silicone oil, long-chain hydroxyl polysiloxane and dialkyl dialkoxy silane.
Further, the main agent comprises the following raw materials in proportion: 100 parts by weight of vinyl polysiloxane, 100-170 parts by weight of MQ resin, 1-15 parts by weight of auxiliary agent, 200-300 parts by weight of solvent and 0.1-0.7 part by weight of inhibitor.
Further, the M/Q ratio of the methyl MQ resin is 0.6-1.0.
Further, the vinyl MQ resin has an M/Q ratio of 0.6 to 1.0 and a vinyl content of 0.5 to 1.5wt%.
Further, the solvent is a conventional solvent such as at least one of toluene, xylene, ethyl acetate, petroleum ether, and mineral spirits.
Further, the inhibitor is at least one of methyl ethyl alcohol, methyl butyl alcohol, ethynyl cyclohexanol, phenyl butyl alcohol, tetramethyl tetravinyl cyclotetrasiloxane, divinyl tetramethyl disiloxane and the like.
Further, the main agent component is prepared by the following method: uniformly mixing vinyl polysiloxane, MQ resin, an auxiliary agent and a solvent, stirring for 3-5 hours at 80-120 ℃, and cooling to below 50 ℃; and mixing with inhibitor, and stirring to obtain the final product.
Further, the proportion of each component in the organic silicon pressure-sensitive adhesive is as follows: 100 parts by weight of main agent component, 1.0-2.0 parts by weight of catalyst component, 1.2-2.0 parts by weight of cross-linking agent component and 0.8-1.2 parts by weight of anchoring agent component.
Further, the catalyst component is a platinum metal catalyst with a platinum content of 4000-6000 ppm.
Further, the cross-linking agent component is hydrogen polysiloxane with the hydrogen group content of 1.2-1.6 wt%.
Further, the anchoring agent component is siloxane containing hydrogen groups and epoxy groups and containing hydrogen groups and ether groups.
Still further, the anchoring agent component is selected from the group consisting of those represented by the following structural formulas:
Figure BDA0003641916410000031
wherein H is hydrogen, R 1 ，R 2 Is methyl or epoxy-containing, R 3 Is epoxy or epoxy-containing, x, y and z are natural numbers greater than 0, x is more than or equal to 2 and less than or equal to 6, y is more than or equal to 4 and less than or equal to 24,2, and z is more than or equal to 8.
Still further, the anchoring agent component is selected from the following structural formulaSubstances of the structure shown (hydro polysiloxanes):
Figure BDA0003641916410000032
wherein H is hydrogen; m and n are natural numbers; wherein m is more than or equal to 30 and less than or equal to 70, n is more than or equal to 0 and less than or equal to 10.
Furthermore, when the organic silicon pressure-sensitive adhesive is matched with a fluorine release film (the fluorine release film is a release film which is the main stream in China), the film tearing force is less than or equal to 3.5g/25mm.
The second technical problem to be solved by the invention is to provide a preparation method of the organic silicon pressure-sensitive adhesive, which comprises the following steps: the main agent component, the cross-linking agent component, the anchoring agent component and the catalyst component are prepared into the organic silicon pressure-sensitive adhesive by adopting a method for preparing the pressure-sensitive adhesive; wherein, the raw materials of the main agent component comprise: vinyl polysiloxane, MQ resin, auxiliary agent, solvent and inhibitor, wherein the vinyl polysiloxane is composed of 2-20wt% of vinyl polysiloxane with vinyl content of 1.0-2.0wt% and 80-98wt% of vinyl polysiloxane with vinyl content of 0.03-0.2wt%; the MQ resin is composed of 70-90 wt% of methyl MQ resin and 10-30 wt% of vinyl MQ resin.
Further, the preparation method of the organic silicon pressure-sensitive adhesive comprises the following steps:
1) Preparing main agent components: uniformly mixing 100 parts of vinyl polysiloxane, 100-170 parts of MQ resin, 1-15 parts of auxiliary agent and 200-300 parts of solvent, stirring for 3-5 hours at 80-120 ℃, cooling to below 50 ℃, mixing with 0.1-0.7 part of inhibitor, and uniformly stirring;
2) Preparing a pressure-sensitive adhesive: 50-250 parts of diluent is added into 100 parts of main agent components, and the mixture is stirred uniformly; then adding 1.2-2.0 parts of cross-linking agent components under the stirring condition in sequence, and stirring for 2-10 minutes; adding 0.8-1.2 parts of anchoring agent components, and stirring for 2-10 minutes; and finally adding 1.0-2.0 parts of catalyst component, and stirring for 10-20 min to prepare the pressure-sensitive adhesive.
Further, in the preparation method of the organic silicon pressure-sensitive adhesive, the diluent is at least one of ethyl acetate, dimethylbenzene, solvent oil, petroleum ether or cyclohexane.
The third technical problem to be solved by the invention is to indicate the application of the organic silicon pressure-sensitive adhesive in an AF screen protective film, a special interface protective film or an adhesive tape.
The fourth technical problem to be solved by the invention is to provide an AF screen pressure-sensitive adhesive protective film, which is prepared by the following method: uniformly coating the prepared pressure-sensitive adhesive on a substrate, and curing the substrate coated with the pressure-sensitive adhesive at 130-160 ℃ for 1.0-3.0 minutes; and (5) taking out, and coating a fluorine release film to obtain the AF screen pressure-sensitive adhesive protective film.
Further, the AF screen stripping force of the AF screen pressure-sensitive adhesive protective film is more than or equal to 30g/25mm, and the AF screen water drop angle is more than 112 degrees.
Further, the AF screen pressure-sensitive adhesive protective film has an AF screen peeling force variation of not more than 15% after aging for 2 hours at 90 ℃.
Further, fingerprint marks and pause marks of the AF screen pressure-sensitive adhesive protective film can disappear within 15 seconds.
Further, the substrate is a substrate such as a PET film, a PC film, a PE film, a PI film or a TPU film.
Further, in the method, the substrate coated with the pressure-sensitive adhesive is cured for 1.0 to 3.0 minutes by being placed in an oven with the temperature of 130 to 160 ℃ or directly enters a drying tunnel with the highest temperature of 160 ℃ to be cured for 1.0 to 3.0 minutes, so that the AF screen pressure-sensitive adhesive protective film is prepared.
Further, the thickness of the dry adhesive obtained after the pressure-sensitive adhesive is uniformly coated on the base material and solidified is 10-40 mu m.
The fifth technical problem to be solved by the invention is to provide a method for reducing the film tearing force of an organosilicon pressure-sensitive adhesive and a fluorine release film, which comprises the following steps: preparing an organosilicon pressure-sensitive adhesive by selecting a main agent component, a catalyst component, a cross-linking agent component and an anchoring agent component, wherein the main agent component is prepared from the following raw materials: vinyl polysiloxane, MQ resin, auxiliary agent, solvent and inhibitor, wherein the vinyl polysiloxane is composed of 2-20wt% of vinyl polysiloxane with vinyl content of 1.0-2.0wt% and 80-98wt% of vinyl polysiloxane with vinyl content of 0.03-0.2wt%; the MQ resin is composed of 70-90 wt% of methyl MQ resin and 10-30 wt% of vinyl MQ resin.
The sixth technical problem to be solved by the present invention is to provide a method for reducing residence time of pressure sensitive adhesive stop marks and/or fingerprint marks, the method comprising: preparing an organosilicon pressure-sensitive adhesive by selecting a main agent component, a catalyst component, a cross-linking agent component and an anchoring agent component, wherein the raw materials of the main agent component are selected from the following materials: vinyl polysiloxane, MQ resin, auxiliary agent, solvent and inhibitor, wherein the vinyl polysiloxane is composed of 2-20wt% of vinyl polysiloxane with vinyl content of 1.0-2.0wt% and 80-98wt% of vinyl polysiloxane with vinyl content of 0.03-0.2wt%; the MQ resin is composed of 70-90 wt% of methyl MQ resin and 10-30 wt% of vinyl MQ resin.
In the present invention, the parts of the raw materials in the present invention refer to parts by mass unless otherwise specified.
Compared with the conventional addition type organic silicon pressure-sensitive adhesive, the invention has the characteristics that:
1. the conventional addition type organic silicon pressure-sensitive adhesive can select polysiloxane with lower vinyl content as a basic reactant, and simultaneously improves the addition amount of MQ resin to a certain extent as much as possible, so as to improve the stripping force of the pressure-sensitive adhesive to a steel plate; in a certain range, the direction is also applicable to AF screen pressure-sensitive adhesives, but the AF screen stripping force can only be improved to about 15g/25mm, and the AF screen stripping force can not be further improved. The invention adopts polysiloxane with higher vinyl content and polysiloxane with lower vinyl content to match, and greatly reduces the peeling force of the steel plate, but greatly improves the peeling force of the AF screen, and simultaneously ensures the flexibility of the pressure-sensitive adhesive so as to quickly disappear fingerprint.
2. The conventional addition type organic silicon pressure-sensitive adhesive is rarely added with other chain extension auxiliary agents so as not to reduce the bulk strength of the pressure-sensitive adhesive and influence the performance; the chain extender is specially introduced in the invention, so that the initial viscosity of the pressure-sensitive adhesive can be increased, and the film tearing force of the fluorine release film can be reduced, thereby achieving the effect of good matching with the fluorine release film.
3. In the invention, in addition to the MQ resin, the MQ resin is adopted to improve the stripping force, and partial vinyl MQ resin with lower vinyl content is additionally added, so that the stripping force of the pressure-sensitive adhesive AF screen and the aging stability of the stripping force of the pressure-sensitive adhesive AF screen are improved.
4. The anchoring agent is an auxiliary agent necessary for the use of the pressure-sensitive adhesive, and generally adopts alkoxy, acyloxy, epoxy and other groups of silane coupling agents or related modified products as the anchoring agent; in the aging process, especially under the condition of higher temperature, partial unreacted groups in the anchoring agent can continuously react, so that the film tearing force is continuously increased, therefore, the invention adopts siloxane as a main body and adopts the anchoring agent with a small amount of hydrogen groups and epoxy groups, wherein the hydrogen groups can participate in the reaction to improve the stability of the pressure-sensitive adhesive, the epoxy groups have the adhesiveness with a base material, and the pressure-sensitive adhesive and the base material are well bonded.
5. The organic silicon pressure-sensitive adhesive has the advantages that the organic silicon pressure-sensitive adhesive is matched with a domestic main stream fluorine release film, and the film tearing force is less than or equal to 3.5g/25mm; the peeling force of the AF screen is more than or equal to 30g/25mm (the water drop angle of the AF screen is more than 112 degrees); aging at 90deg.C for 2 hr to prevent the AF screen from peeling force from changing by 15%; fingerprint marks and pause marks can disappear within 15 seconds, and the like, and can be widely applied to the application field of AF screen protection films in the mobile phone or display industry.
Detailed Description
The invention provides an organic silicon pressure-sensitive adhesive, which comprises a main agent component, a catalyst component, a cross-linking agent component and an anchoring agent component; and the main agent component comprises the following raw materials: vinyl polysiloxane, MQ resin, auxiliary agent, solvent and inhibitor, wherein the vinyl polysiloxane is composed of 2-20wt% of vinyl polysiloxane with vinyl content of 1.0-2.0wt% and 80-98wt% of vinyl polysiloxane with vinyl content of 0.03-0.2wt%; the MQ resin is a mixture of 70-90 wt% of methyl MQ resin and 10-30 wt% of vinyl MQ resin.
In the invention, the vinyl polysiloxane in the main component consists of two types of vinyl polysiloxane, wherein one type of vinyl polysiloxane is vinyl polysiloxane with the vinyl content of 1.0-2.0 wt% and the other type of vinyl polysiloxane is vinyl polysiloxane with the vinyl content of 0.03-0.2 wt%; vinyl polysiloxane with the vinyl content of 0.6-2.0 wt% accounts for 2-20 wt% of the total amount of the vinyl polysiloxane, and vinyl polysiloxane with the vinyl content of 0.03-0.2 wt% accounts for 80-98 wt% of the total amount of the vinyl polysiloxane. The MQ resin is a mixture of methyl MQ resin and vinyl MQ resin; wherein the methyl MQ resin accounts for 70-90 wt% of the total amount of the MQ resin, and the vinyl MQ resin accounts for 10-30 wt% of the total amount of the MQ resin. The invention adopts polysiloxane with higher vinyl content and polysiloxane with lower vinyl content to match and use, and can greatly improve the peeling force of the AF screen while greatly reducing the peeling force of the steel plate, and simultaneously ensure the flexibility of the pressure-sensitive adhesive so as to ensure that fingerprint marks disappear rapidly.
The invention also provides an AF screen protection film, which is prepared by the following method: firstly, uniformly mixing a main agent component, a cross-linking agent component, an anchoring agent component and a diluting solvent, and finally adding a catalyst component, and uniformly mixing to obtain a pressure-sensitive adhesive; and coating the mixed pressure-sensitive adhesive on a base material (PET film, PC film, PE film or TPU film and the like), and curing under a certain temperature condition.
The invention aims to improve the peeling force of an AF screen, and the existing method for improving the peeling force of the AF screen mainly comprises 3 methods: (1) The ratio of MQ resin is increased to a certain extent as the conventional addition type organic silicon pressure-sensitive adhesive, the addition of MQ resin is high, the stripping force of a steel plate can be high, and the stripping force of an AF screen can be relatively high; however, when the amount of the MQ resin added reaches a certain value, the peel force decreases. (2) similar principle: the AF screen surface is a layer of fluorine modified paint with compact structure, the surface density is high, and the crosslinking degree of the pressure-sensitive adhesive is properly improved according to a similar principle, so that the AF screen stripping force can be improved to a certain extent. (3) principle of primary adhesion: by improving the primary adhesion of the pressure-sensitive adhesive, the adsorptivity between the pressure-sensitive adhesive and AF can be improved, thereby improving the AF stripping force.
The above 3 methods for improving the peeling force of the AF screen have the defects: the adding amount of the MQ resin can only reach about 15g/25mm at most when simply improving the AF screen stripping force; the AF screen stripping force can be improved by improving the crosslinking degree, but the property of the AF screen after aging can be obviously changed due to the incomplete short-time reaction due to the large increase of the number of the reactive groups, and the matching property with a release film can be poor and the film stripping force can be increased along with the increase of the crosslinking degree; the primary adhesion is generally realized by incomplete curing or increasing the hydroxyl content in the resin, the incomplete curing can lead to long or no disappearance of fingerprint and pause mark, the aging stability of the pressure-sensitive adhesive is poor, and the increase of the hydroxyl content of the resin directly leads to unstable product performance.
In order to solve the problems, the invention adopts the following scheme:
1. the AF screen stripping force is improved by adopting the mode of increasing the resin addition amount and improving the reaction crosslinking degree of the pressure-sensitive adhesive, namely the mode of improving the reaction crosslinking degree of the pressure-sensitive adhesive is to improve the content of vinyl groups in the auxiliary component, wherein one part of the vinyl groups are embodied in vinyl polysiloxane, and the other part of the vinyl groups are embodied in vinyl MQ resin; if vinyl polysiloxane with higher vinyl content is adopted, the crosslinking degree of the pressure-sensitive adhesive after curing is overlarge, the colloid strength is low, the problem that fingerprint marks cannot disappear can occur, and meanwhile, the original viscosity of the pressure-sensitive adhesive is reduced too much to reduce the peeling force of an AF screen; moreover, an excessive amount of polysiloxane having a high vinyl content may cause a low degree of reaction of vinyl groups, resulting in poor aging stability in the latter stage; therefore, the vinyl polysiloxane with low vinyl content is used as a reaction main body of the pressure-sensitive adhesive, so that the body strength of the pressure-sensitive adhesive can be ensured, and meanwhile, the fingerprint mark and the pause mark can be ensured to disappear rapidly; meanwhile, the aging stability of the pressure-sensitive adhesive is better.
2. The invention adopts the vinyl MQ resin with low vinyl content and the methyl MQ resin to be matched for use, can assist in increasing the reaction crosslinking degree of the pressure-sensitive adhesive to improve the AF stripping force, and has the effect of improving the strength of the pressure-sensitive adhesive body after curing because vinyl groups in the vinyl MQ resin can participate in reaction.
3. The chain extender is added, so that the initial viscosity of the pressure-sensitive adhesive can be improved, and the film tearing force of the fluorine-containing release film is reduced, so that the effect of good matching with the fluorine-containing release film is achieved; however, the addition of the auxiliary agent results in a decrease in bulk strength of the pressure sensitive adhesive, which may lead to the appearance of a noticeable dead print, and the addition of the low vinyl content vinyl MQ resin helps to mitigate the dead print.
4. The invention adopts siloxane as a main body, and contains a small amount of anchoring agent of hydrogen groups and epoxy groups, wherein the hydrogen groups can participate in addition reaction, so that the aging stability of the pressure-sensitive adhesive is improved; the epoxy group has adhesion with the substrate, so that the pressure-sensitive adhesive is well adhered with the substrate.
The following description of the embodiments of the present invention will clearly and fully illustrate the embodiments of the invention that are applicable to an AF screen protective film, and it is apparent that the embodiments described are only some, but not all, of the embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The method for preparing the silicone pressure-sensitive adhesive for an AF screen protective film according to the present invention is described in detail below by way of specific examples, each of which is exemplified by a silicone pressure-sensitive adhesive comprising a main agent component, a catalyst component, an anchor agent component and a crosslinking agent component. In the examples, all parts are by weight unless otherwise indicated.
Example 1:
1) Preparing main agent components: 100 parts of vinyl polysiloxane (wherein the addition amount of vinyl polysiloxane with the vinyl content of 1.0wt% is 2 parts; the addition amount of vinyl polysiloxane with the vinyl content of 0.2wt% is 98 parts), 170 parts of MQ resin (wherein 150 parts of methyl MQ resin and 20 parts of vinyl MQ resin with the vinyl content of 0.5 wt%) are uniformly mixed, 1 part of long-chain alkyl silicone oil and 300 parts of toluene are stirred for 3 hours under the condition of 120 ℃, cooled to below 50 ℃, and then mixed with 0.1 part of ethynyl cyclohexanol, and uniformly stirred;
3) Preparing a pressure-sensitive adhesive: adding 200 parts of diluent ethyl acetate into 100 parts of main agent, and uniformly stirring; then adding 1.2 parts of cross-linking agent component under stirring in sequence, and stirring for 5 minutes; then adding 1.2 parts of anchoring agent component, and stirring for 5 minutes; finally, 1.0 part of catalyst component (Pt content: 5000 PCm) was added and stirred for 10 minutes.
4) Curing of the pressure sensitive adhesive: and (3) coating the prepared pressure-sensitive adhesive on a PET film, coating the PET film to a thickness of 40 mu m, putting the coated substrate into a 160 ℃ oven for curing for 3.0 minutes, taking out, and covering a fluorine release film to obtain the AF screen pressure-sensitive adhesive protective film.
5) Performance test: the main agent components of the pressure-sensitive adhesive, the prepared pressure-sensitive adhesive and the cured pressure-sensitive adhesive protective film were tested, and the performance parameters thereof are shown in table 1.
Example 2:
1) Preparing main agent components: 100 parts of vinyl polysiloxane (wherein the addition amount of vinyl polysiloxane with the vinyl content of 2.0wt% is 7 parts; the addition amount of vinyl polysiloxane with the vinyl content of 0.03wt% is 93 parts), 150 parts of MQ resin (wherein 110 parts of methyl MQ resin and 40 parts of vinyl MQ resin with the vinyl content of 0.5 wt%) are uniformly mixed, 15 parts of hydrogen-containing silicone oil and 250 parts of xylene are uniformly stirred at 120 ℃ for 3 hours, cooled to below 50 ℃, and then mixed with 0.2 part of butynol and 0.5 part of tetramethyl tetra-ethylene cyclotetra-siloxane, and uniformly stirred;
3) Preparing a pressure-sensitive adhesive: adding 200 parts of diluent ethyl acetate into 100 parts of main agent, and uniformly stirring; then adding 2.0 parts of cross-linking agent components under the stirring condition in sequence, and stirring for 5 minutes; then adding 1.2 parts of anchoring agent component, and stirring for 5 minutes; finally, 1.0 part of catalyst component (Pt content is 5000 PCm) is added and stirred for 10 to 20 minutes.
4) Curing of the pressure sensitive adhesive: coating the prepared pressure-sensitive adhesive on a TPU film with the coating thickness of 10 mu m, then placing the coated substrate in a baking oven at 130 ℃ for curing for 2.0 minutes, taking out, and covering a fluorine release film to obtain the AF screen pressure-sensitive adhesive protective film.
5) Performance test: the main agent components of the pressure-sensitive adhesive, the prepared pressure-sensitive adhesive and the cured pressure-sensitive adhesive protective film were tested, and the performance parameters thereof are shown in table 1..
Example 3:
1) Preparing main agent components: 100 parts of vinyl polysiloxane (wherein the addition amount of vinyl polysiloxane with the vinyl content of 1.2 weight percent is 10 parts; the addition amount of vinyl polysiloxane with the vinyl content of 0.16 weight percent is 90 parts), 160 parts of MQ resin (wherein 144 parts of methyl MQ resin and 16 parts of vinyl MQ resin with the vinyl content of 1.5 weight percent) 5 parts of diethyl diethoxy silane and 300 parts of ethyl acetate are uniformly mixed, stirred for 5 hours at 80 ℃, cooled to below 50 ℃, and then mixed with 0.4 part of methyl butynol, and uniformly stirred;
3) Preparing a pressure-sensitive adhesive: adding 200 parts of diluent ethyl acetate into 100 parts of main agent, and uniformly stirring; then adding 1.5 parts of cross-linking agent component under stirring in sequence, and stirring for 5 minutes; then adding 1.0 part of anchoring agent component, and stirring for 5 minutes; finally, 1.6 parts of a catalyst component (Pt content: 5000 PCm) was added and stirred for 10 minutes.
4) Curing of the pressure sensitive adhesive: and (3) coating the prepared pressure-sensitive adhesive on a PC film, wherein the thickness of the coated dry adhesive is 30 mu m, then placing the coated substrate in a 140 ℃ oven for curing for 2.0 minutes, taking out, and coating a fluorine release film to obtain the AF screen pressure-sensitive adhesive protective film.
5) Performance test: the main agent components of the pressure-sensitive adhesive, the prepared pressure-sensitive adhesive and the cured pressure-sensitive adhesive protective film were tested, and the performance parameters thereof are shown in table 1.
Example 4:
1) Preparing main agent components: 100 parts of vinyl polysiloxane (wherein the addition amount of vinyl polysiloxane with the vinyl content of 1.6 weight percent is 10 parts; the addition amount of vinyl polysiloxane with the vinyl content of 0.1 weight percent is 90 parts), 100 parts of MQ resin (wherein 90 parts of methyl MQ resin and 10 parts of vinyl MQ resin with the vinyl content of 1.0 weight percent) 15 parts of 5-kilocs of hydroxy polysiloxane and 300 parts of petroleum ether are uniformly mixed, stirred for 5 hours at 80 ℃, cooled to below 50 ℃, and then mixed with 0.3 part of phenylbutynol, and uniformly stirred;
3) Preparing a pressure-sensitive adhesive: adding 200 parts of diluent ethyl acetate into 100 parts of main agent, and uniformly stirring; then adding 1.5 parts of cross-linking agent component under stirring in sequence, and stirring for 5 minutes; then adding 1.0 part of anchoring agent component, and stirring for 5 minutes; finally, 1.5 parts of a catalyst component (Pt content 4000 PCm) was added and stirred for 10 minutes.
4) Curing of the pressure sensitive adhesive: and (3) coating the prepared pressure-sensitive adhesive on a PET film, wherein the thickness of the coated dry adhesive is 30 mu m, then placing the coated substrate in a 160 ℃ oven for curing for 2.0 minutes, taking out, and coating a fluorine release film to obtain the AF screen pressure-sensitive adhesive protective film.
5) Performance test: the main agent components of the pressure-sensitive adhesive, the prepared pressure-sensitive adhesive and the cured pressure-sensitive adhesive protective film were tested, and the performance parameters thereof are shown in table 1.
Example 5:
1) Preparing main agent components: 100 parts of vinyl polysiloxane (wherein the addition amount of vinyl polysiloxane with the vinyl content of 2.0wt% is 20 parts; the addition amount of vinyl polysiloxane with the vinyl content of 0.04wt% is 80 parts), 170 parts of MQ resin (wherein the methyl MQ resin is 150 parts, the vinyl content of 1.0wt% is 20 parts), 10 parts of long-chain alkyl silicone oil, 200 parts of toluene and 50 parts of ethyl acetate are uniformly mixed, stirred for 4 hours at 100 ℃, cooled to below 50 ℃, and then mixed with 0.3 part of methyl acetylene alcohol and 0.3 part of divinyl tetramethyl disiloxane, and uniformly stirred;
3) Preparing a pressure-sensitive adhesive: adding 200 parts of diluent ethyl acetate into 100 parts of main agent, and uniformly stirring; then adding 1.2 parts of cross-linking agent component under stirring in sequence, and stirring for 5 minutes; then adding 1.2 parts of anchoring agent component, and stirring for 5 minutes; finally, 2.0 parts of catalyst component (Pt content is 4000 PCm) is added and stirred for 10 to 20 minutes.
4) Curing of the pressure sensitive adhesive: and (3) coating the prepared pressure-sensitive adhesive on a PTU film, wherein the thickness of the coated dry adhesive is 15 mu m, then placing the coated substrate in a baking oven at 130 ℃ for curing for 1.0 min, taking out, and coating a fluorine release film to obtain the AF screen pressure-sensitive adhesive protective film.
5) Performance test: the main agent components of the pressure-sensitive adhesive, the prepared pressure-sensitive adhesive and the cured pressure-sensitive adhesive protective film were tested, and the performance parameters thereof are shown in table 1.
Comparative example 1:
1) Preparing main agent components: 100 parts of vinyl polysiloxane (wherein the addition amount of vinyl polysiloxane with the vinyl content of 2.0wt% is 25 parts; the addition amount of vinyl polysiloxane with the vinyl content of 0.03-0.2 wt% is 75 parts), 170 parts of MQ resin (wherein 150 parts of methyl MQ resin and 20 parts of vinyl MQ resin with the vinyl content of 1.0 wt%) are uniformly mixed, 1 part of long-chain alkyl silicone oil and 300 parts of toluene are stirred for 3 hours under the condition of 120 ℃, cooled to below 50 ℃, and then mixed with 0.1 part of ethynyl cyclohexanol, and uniformly stirred;
3) Preparing a pressure-sensitive adhesive: adding 200 parts of diluent ethyl acetate into 100 parts of main agent, and uniformly stirring; then adding 1.2 parts of cross-linking agent component under stirring in sequence, and stirring for 5 minutes; then adding 1.2 parts of anchoring agent component, and stirring for 5 minutes; finally, 1.0 part of catalyst component (Pt content: 5000 PCm) was added and stirred for 10 minutes.
4) Curing of the pressure sensitive adhesive: and (3) coating the prepared pressure-sensitive adhesive on a PET film, coating the PET film to a thickness of 40 mu m, putting the coated substrate into a 160 ℃ oven for curing for 3.0 minutes, taking out, and covering a fluorine release film to obtain the AF screen pressure-sensitive adhesive protective film.
5) Performance test: the main agent components of the pressure-sensitive adhesive, the prepared pressure-sensitive adhesive and the cured pressure-sensitive adhesive protective film were tested, and the performance parameters thereof are shown in table 1.
Comparative example 2
1) Preparing main agent components: 100 parts of vinyl polysiloxane (wherein the addition amount of vinyl polysiloxane with the vinyl content of 3.0wt% is 2 parts; the addition amount of vinyl polysiloxane with the vinyl content of 0.2wt% is 98 parts), 170 parts of MQ resin (wherein 150 parts of methyl MQ resin and 20 parts of vinyl MQ resin with the vinyl content of 0.5 wt%) are uniformly mixed, 1 part of long-chain alkyl silicone oil and 300 parts of toluene are stirred for 3 hours under the condition of 120 ℃, cooled to below 50 ℃, and then mixed with 0.1 part of ethynyl cyclohexanol, and uniformly stirred;
3) Preparing a pressure-sensitive adhesive: adding 200 parts of diluent ethyl acetate into 100 parts of main agent, and uniformly stirring; then adding 1.2 parts of cross-linking agent component under stirring in sequence, and stirring for 5 minutes; then adding 1.2 parts of anchoring agent component, and stirring for 5 minutes; finally, 1.0 part of catalyst component (Pt content: 5000 PCm) was added and stirred for 10 minutes.
4) Curing of the pressure sensitive adhesive: and (3) coating the prepared pressure-sensitive adhesive on a PET film, coating the PET film to a thickness of 40 mu m, putting the coated substrate into a 160 ℃ oven for curing for 3.0 minutes, taking out, and covering a fluorine release film to obtain the AF screen pressure-sensitive adhesive protective film.
5) Performance test: the main agent components of the pressure-sensitive adhesive, the prepared pressure-sensitive adhesive and the cured pressure-sensitive adhesive protective film were tested, and the performance parameters thereof are shown in table 1.
Comparative example 3
1) Preparing main agent components: 100 parts of vinyl polysiloxane (wherein the addition amount of vinyl polysiloxane with the vinyl content of 1.0wt% is 2 parts; the addition amount of vinyl polysiloxane with the vinyl content of 0.2wt% is 98 parts), 170 parts of MQ resin (wherein 150 parts of methyl MQ resin and 20 parts of vinyl MQ resin with the vinyl content of 0.5 wt%) and 300 parts of toluene are uniformly mixed, stirred for 3 hours at 120 ℃, cooled to below 50 ℃, and then mixed with 0.1 part of ethynyl cyclohexanol, and uniformly stirred;
3) Preparing a pressure-sensitive adhesive: adding 200 parts of diluent ethyl acetate into 100 parts of main agent, and uniformly stirring; then adding 1.2 parts of cross-linking agent component under stirring in sequence, and stirring for 5 minutes; then adding 1.2 parts of anchoring agent component, and stirring for 5 minutes; finally, 1.0 part of catalyst component (Pt content: 5000 PCm) was added and stirred for 10 minutes.
4) Curing of the pressure sensitive adhesive: and (3) coating the prepared pressure-sensitive adhesive on a PET film, coating the PET film to a thickness of 40 mu m, putting the coated substrate into a 160 ℃ oven for curing for 3.0 minutes, taking out, and covering a fluorine release film to obtain the AF screen pressure-sensitive adhesive protective film.
5) Performance test: the main agent components of the pressure-sensitive adhesive, the prepared pressure-sensitive adhesive and the cured pressure-sensitive adhesive protective film were tested, and the performance parameters thereof are shown in table 1.
Comparative example 4
Preparing main agent components: 100 parts of vinyl polysiloxane (wherein the addition amount of vinyl polysiloxane with the vinyl content of 1.0wt% is 2 parts, and the addition amount of vinyl polysiloxane with the vinyl content of 0.2wt% is 98 parts), 170 parts of MQ resin (wherein the resin is all methyl MQ resin), 1 part of long-chain alkyl silicone oil and 300 parts of toluene are uniformly mixed, stirred for 3 hours at 120 ℃, cooled to below 50 ℃, then mixed with 0.1 part of ethynyl cyclohexanol, and uniformly stirred;
3) Preparing a pressure-sensitive adhesive: adding 200 parts of diluent ethyl acetate into 100 parts of main agent, and uniformly stirring; then adding 1.2 parts of cross-linking agent component under stirring in sequence, and stirring for 5 minutes; then adding 1.2 parts of anchoring agent component, and stirring for 5 minutes; finally, 1.0 part of catalyst component (Pt content: 5000 PCm) was added and stirred for 10 minutes.
4) Curing of the pressure sensitive adhesive: and (3) coating the prepared pressure-sensitive adhesive on a PET film, coating the PET film to a thickness of 40 mu m, putting the coated substrate into a 160 ℃ oven for curing for 3.0 minutes, taking out, and covering a fluorine release film to obtain the AF screen pressure-sensitive adhesive protective film.
5) Performance test: the main agent components of the pressure-sensitive adhesive, the prepared pressure-sensitive adhesive and the cured pressure-sensitive adhesive protective film were tested, and the performance parameters thereof are shown in table 1.
In the embodiment of the invention, the detection standard and the detection method adopted for the detection of the performance of the organic silicon pressure-sensitive adhesive are as follows:
the AF screen peeling force detection method refers to a 180-degree peeling strength test method in GB/T2792, and an experimental plate is replaced by an AF screen with a water drop angle of more than 112 degrees.
The film tearing force testing method comprises the following steps: and selecting a standard experiment plate according to GB/T2792, cutting a double-sided adhesive tape with the same size as the standard experiment plate, tearing a layer of isolation film, flatly pasting the whole double-sided adhesive tape on the standard experiment plate, and tearing the isolation film on the upper surface of the double-sided adhesive tape. A sample is prepared in reference GB/T2792, the substrate surface (non-fluoride release film surface) of the sample is flatly adhered to a standard test board with double faced adhesive tape, and the fluoride release film is torn by reference to a 180-degree peel strength test method in the reference GB/T2792, and the obtained force is film tearing force.
The aging performance testing method comprises the following steps: after aging the pressure-sensitive adhesive protective film at 90 ℃ for 2 hours, the AF screen peeling force was again tested. The data obtained are the AF screen peel force after aging and the tear force after aging. (post-aging data-pre-aging data)/pre-aging data are 100% absolute values +.15%.
Fingerprint mark: the pressure-sensitive adhesive protective film is stuck on an AF screen, and a trace of about 2cm is marked on the surface layer of the protective film by using a pencil hardness meter (2B pencil), and the trace can disappear in 15 seconds after timing observation.
Pause printing: and (3) attaching the pressure-sensitive adhesive protective film to an AF screen, tearing at a constant speed for 4-5cm, stopping for 10 seconds, tearing again, and timing and observing to ensure that marks at the time of stopping can disappear within 15 seconds.
TABLE 1 results of Performance measurements for examples 1-6
Figure BDA0003641916410000121
As can be seen from examples 1 to 5 in Table 1, within the scope of the present invention, the AF screen peeling force, the film tearing force, the fingerprint mark, the stop mark and the like all meet the index requirements, the aging performance is stable, and the fluctuation range before and after aging is far less than 15%.
In addition, as is clear from table 1, in example 1, when the high vinyl content polysiloxane is out of the range required by the present invention, the film tearing force is greatly improved, and the reaction proceeds further due to the excessively high vinyl content, and the AF screen peeling force is greatly reduced after aging. Example 1 differs from comparative example 2 only in the vinyl content of the high vinyl content polysiloxane, and when the vinyl content of the high vinyl content polysiloxane is > 2%, the stability after aging is deteriorated. Example 1 differs from comparative example 3 in that only the chain extender is used, and in comparative example 3, no chain extender is added, and the AF flat peeling force is significantly reduced, and at the same time, the stop mark disappearance time is shortened. Example 1 differs from comparative example 4 in that only the vinyl MQ resin was added, and in comparative example 4, no vinyl MQ resin was added, and the AF screen peel force was significantly reduced and the film tearing force was significantly increased; simultaneously; fingerprint and dwell time are significantly longer.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.

Claims (25)

1. The organic silicon pressure-sensitive adhesive is characterized by comprising a main agent component, a catalyst component, a cross-linking agent component and an anchoring agent component; the main agent comprises the following raw materials: vinyl polysiloxane, MQ resin, auxiliary agent, solvent and inhibitor, wherein the vinyl polysiloxane is composed of 2-20wt% of vinyl polysiloxane with vinyl content of 1.0-2.0wt% and 80-98wt% of vinyl polysiloxane with vinyl content of 0.03-0.2wt%; the MQ resin consists of 70-90 wt% of methyl MQ resin and 10-30 wt% of vinyl MQ resin; the auxiliary agent is at least one of long-chain alkyl silicone oil, hydrogen-terminated silicone oil, long-chain hydroxyl polysiloxane or dialkyl dialkoxy silane;
And the main agent comprises the following raw materials in proportion: 100 parts by weight of vinyl polysiloxane, 100-170 parts by weight of MQ resin, 1-15 parts by weight of auxiliary agent, 200-300 parts by weight of solvent and 0.1-0.7 part by weight of inhibitor.
2. The silicone pressure sensitive adhesive of claim 1, wherein the solvent is at least one of toluene, xylene, ethyl acetate, petroleum ether, or mineral spirits.
3. The silicone pressure sensitive adhesive of claim 1, wherein the inhibitor is at least one of methyl ethyl alcohol, methyl butyl alcohol, ethynyl cyclohexanol, phenyl butyl alcohol, tetramethyl tetra vinyl cyclotetrasiloxane, or divinyl tetramethyl disiloxane.
4. The silicone pressure sensitive adhesive according to claim 1 or 2, wherein the main agent component is prepared by the following method: uniformly mixing vinyl polysiloxane, MQ resin, an auxiliary agent and a solvent, stirring for 3-5 hours at 80-120 ℃, and cooling to below 50 ℃; and mixing with the inhibitor, and stirring uniformly to obtain the main agent component.
5. The silicone pressure-sensitive adhesive according to claim 1 or 2, wherein the methyl MQ resin has an M/Q ratio of 0.6 to 1.0.
6. The silicone pressure-sensitive adhesive according to claim 1 or 2, wherein the vinyl MQ resin has an M/Q ratio of 0.6 to 1.0 and a vinyl content of 0.5 to 1.5wt%.
7. The organic silicon pressure-sensitive adhesive according to any one of claims 1 to 3, wherein the organic silicon pressure-sensitive adhesive comprises the following components in proportion: 100 parts by weight of main agent component, 1.0-2.0 parts by weight of catalyst component, 1.2-2.0 parts by weight of cross-linking agent component and 0.8-1.2 parts by weight of anchoring agent component.
8. The silicone pressure-sensitive adhesive according to claim 7, wherein the catalyst component is a platinum metal catalyst having a platinum content of 4000 to 6000 ppm.
9. The silicone pressure sensitive adhesive of claim 7, wherein the crosslinker component is a hydrogen-based polysiloxane having a hydrogen content of 1.2 to 1.6 wt%.
10. The silicone pressure sensitive adhesive of claim 7, wherein the anchor component is a silicone containing hydrogen and epoxy functional groups, a silicone containing hydrogen and ether functional groups.
11. The silicone pressure sensitive adhesive of claim 10, wherein the anchor component is selected from the group consisting of:
Figure QLYQS_1
Wherein R is 1 ，R 2 Is methyl or epoxy-containing, R 3 Is epoxy or epoxy-containing group, x is more than or equal to 2 and less than or equal to 6, y is more than or equal to 4 and less than or equal to 24,2, and z is more than or equal to 8.
12. An organosilicon pressure-sensitive adhesive according to any one of claims 1-3, wherein when the organosilicon pressure-sensitive adhesive is used in combination with a fluorine release film, the film tearing force is less than or equal to 3.5g/25mm.
13. The method for preparing the organic silicon pressure-sensitive adhesive as claimed in any one of claims 1 to 12, wherein the preparation method comprises the following steps: the main agent component, the cross-linking agent component, the anchoring agent component and the catalyst component are prepared into the organic silicon pressure-sensitive adhesive by adopting a method for preparing the pressure-sensitive adhesive; wherein, the raw materials of the main agent component comprise: vinyl polysiloxane, MQ resin, auxiliary agent, solvent and inhibitor, wherein the vinyl polysiloxane is composed of 2-20wt% of vinyl polysiloxane with vinyl content of 1.0-2.0wt% and 80-98wt% of vinyl polysiloxane with vinyl content of 0.03-0.2wt%; the MQ resin is composed of 70-90 wt% of methyl MQ resin and 10-30 wt% of vinyl MQ resin.
14. The method for preparing the organic silicon pressure-sensitive adhesive according to claim 13, wherein the method for preparing the organic silicon pressure-sensitive adhesive comprises the following steps:
1) Preparing main agent components: uniformly mixing 100 parts of vinyl polysiloxane, 100-170 parts of MQ resin, 1-15 parts of auxiliary agent and 200-300 parts of solvent, stirring for 3-5 hours at 80-120 ℃, cooling to below 50 ℃, mixing with 0.1-0.7 part of inhibitor, and uniformly stirring;
2) Preparing a pressure-sensitive adhesive: 50-250 parts of diluent is added into 100 parts of main agent components, and the mixture is stirred uniformly; then adding 1.2-2.0 parts of cross-linking agent components under the stirring condition in sequence, and stirring for 2-10 minutes; adding 0.8-1.2 parts of anchoring agent components, and stirring for 2-10 minutes; and finally adding 1.0-2.0 parts of catalyst component, and stirring for 10-20 min to prepare the pressure-sensitive adhesive.
15. The method for preparing an organic silicon pressure-sensitive adhesive according to claim 14, wherein in the step 2), the diluent is at least one of ethyl acetate, xylene, solvent oil, petroleum ether or cyclohexane.
16. The use of an organosilicon pressure-sensitive adhesive in an AF screen protective film, a special interface protective film or an adhesive tape, which is the pressure-sensitive adhesive according to any one of claims 1 to 12 or the pressure-sensitive adhesive produced by the production method according to any one of claims 13 to 15.
17. The AF screen pressure-sensitive adhesive protective film is characterized by being prepared by the following method: firstly, uniformly coating the pressure-sensitive adhesive on a substrate, and then curing the substrate coated with the pressure-sensitive adhesive at 130-160 ℃ for 1.0-3.0 minutes; coating a fluorine release film after taking out to obtain an AF screen pressure-sensitive adhesive protective film; wherein the pressure-sensitive adhesive is the pressure-sensitive adhesive according to any one of claims 1 to 12, or the pressure-sensitive adhesive prepared by the preparation method according to any one of claims 13 to 15.
18. The AF screen pressure-sensitive adhesive protective film according to claim 17, wherein said substrate is a PET film, a PC film, a PE film, a PI film, or a TPU film.
19. The protective film for an AF screen pressure-sensitive adhesive according to claim 17, wherein said method is characterized in that said substrate coated with the pressure-sensitive adhesive is cured by being placed in an oven at 130 to 160 ℃ for 1.0 to 3.0 minutes or directly put in an oven at 160 ℃ for 1.0 to 3.0 minutes to prepare the protective film for an AF screen pressure-sensitive adhesive.
20. The protective film for an AF screen pressure-sensitive adhesive as claimed in claim 17, wherein the thickness of the dry adhesive obtained after the pressure-sensitive adhesive is uniformly coated on the substrate and cured is 10 to 40 μm.
21. The AF screen pressure-sensitive adhesive protective film according to claim 17, wherein the AF screen pressure-sensitive adhesive protective film has an AF screen peeling force of not less than 30g/25mm and an AF screen water drop angle of > 112 °.
22. The AF screen pressure-sensitive adhesive protective film according to claim 17, wherein said AF screen pressure-sensitive adhesive protective film has an AF screen peel force variation of not more than 15% after aging for 2 hours at 90 ℃.
23. The AF screen pressure-sensitive adhesive protective film according to claim 17, wherein fingerprint marks and pause marks of said AF screen pressure-sensitive adhesive protective film disappear within 15 seconds.
24. A method for reducing film tearing force of an organosilicon pressure-sensitive adhesive and a fluorine release film is characterized by comprising the following steps: preparing an organosilicon pressure-sensitive adhesive by selecting a main agent component, a catalyst component, a cross-linking agent component and an anchoring agent component, wherein the raw materials of the main agent component are selected from the following materials: vinyl polysiloxane, MQ resin, auxiliary agent, solvent and inhibitor, wherein the vinyl polysiloxane is composed of 2-20wt% of vinyl polysiloxane with vinyl content of 1.0-2.0wt% and 80-98wt% of vinyl polysiloxane with vinyl content of 0.03-0.2wt%; the MQ resin consists of 70-90 wt% of methyl MQ resin and 10-30 wt% of vinyl MQ resin; the auxiliary agent is at least one of long-chain alkyl silicone oil, hydrogen-terminated silicone oil, long-chain hydroxyl polysiloxane or dialkyl dialkoxy silane; and the main agent comprises the following raw materials in proportion: 100 parts by weight of vinyl polysiloxane, 100-170 parts by weight of MQ resin, 1-15 parts by weight of auxiliary agent, 200-300 parts by weight of solvent and 0.1-0.7 part by weight of inhibitor.
25. A method of reducing dwell time of a pressure sensitive adhesive dwell and/or finger mark, said method comprising: preparing an organosilicon pressure-sensitive adhesive by selecting a main agent component, a catalyst component, a cross-linking agent component and an anchoring agent component, wherein the raw materials of the main agent component are selected from the following materials: vinyl polysiloxane, MQ resin, auxiliary agent, solvent and inhibitor, wherein the vinyl polysiloxane is composed of 2-20wt% of vinyl polysiloxane with vinyl content of 1.0-2.0wt% and 80-98wt% of vinyl polysiloxane with vinyl content of 0.03-0.2wt%; the MQ resin consists of 70-90 wt% of methyl MQ resin and 10-30 wt% of vinyl MQ resin; the auxiliary agent is at least one of long-chain alkyl silicone oil, hydrogen-terminated silicone oil, long-chain hydroxyl polysiloxane or dialkyl dialkoxy silane; and the main agent comprises the following raw materials in proportion: 100 parts by weight of vinyl polysiloxane, 100-170 parts by weight of MQ resin, 1-15 parts by weight of auxiliary agent, 200-300 parts by weight of solvent and 0.1-0.7 part by weight of inhibitor.
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